CN103901157A - Method for continuously and quickly measuring copper and iron in ore leaching solution - Google Patents
Method for continuously and quickly measuring copper and iron in ore leaching solution Download PDFInfo
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- CN103901157A CN103901157A CN201210586485.8A CN201210586485A CN103901157A CN 103901157 A CN103901157 A CN 103901157A CN 201210586485 A CN201210586485 A CN 201210586485A CN 103901157 A CN103901157 A CN 103901157A
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Abstract
The invention discloses a method for continuously and quickly measuring copper and iron in an ore leaching solution. The method comprises the following steps: a, adding an oxidizing agent to 5-10mL of a to-be-measured ore leaching solution, and heating at low temperatures till a volume is 1-2mL; b, cooling to room temperature and then adjusting acidity, adding a masking agent to mask the iron, then adding potassium iodide, and titrating the copper by using a sodium thiosulfate standard solution with starch as an indicator; c, adding a demasking agent into the solution with the titrated copper to demask the iron, and standing; and d, titrating the iron by using the sodium thiosulfate standard solution, and simultaneously analyzing and carrying out reagent blank, thus measuring a volume of the sodium thiosulfate standard solution consumed by iron by subtracting the reagent blank from the volume of the consumed sodium thiosulfate standard solution. The masking agent is an ammonium hydrogen fluoride saturated solution which is used for masking completely with an excessive amount of 0.5-1.0mL; the demasking agent is a hydrochloric acid solution of aluminium trichloride; the adding amount of the demasking agent is 5.0-10.0mL. The method is less in pollution to environment and quick; the operation processes are easy to control and master, and thus the method is relatively applicable to analysis and measurement of the copper and the iron in large-batch ore leaching solution; the result is good in accuracy and precision.
Description
Technical field
The present invention relates to the continuous rapid analysis of copper iron in ore leachate, specifically, relate to a kind of by adding suitable oxidizer treatment ore leachate, the analytical approach of copper iron in iodimetric titration Fast Continuous Determination ore leachate.
Background technology
Nonferrous metallic ores, copper iron is modal element.Wet method is extracted in the process of copper, and the copper iron in the ore leachate in enormous quantities of generation needs to measure rapidly continuously.At present, the assay method of copper mainly contains iodimetric titration, spectrophotometric method, polarography, atomic absorption spectrography (AAS).The assay method of iron mainly contains dichromate method, ceriometry, sulfosalicylic acid photometry, Phen photometry, atomic absorption spectrography (AAS).For the mensuration of copper iron in ore leachate, the assay method that copper is conventional is iodimetric titration, and the assay method that iron is conventional is dichromate method.Iodimetric Determination of Copper:, by adding appropriate nitric acid, sulfuric acid, on electric furnace, heating evaporation to the white cigarette of sulfuric anhydride emits most processing ore leachate.The strong acid treatment ore leachate time is long, environmental pollution is serious, is not suitable for the express-analysis of ore leachate in enormous quantities.Dichromate method is surveyed iron, although ore leachate is without processing, but also need to reduce after most of ferric iron and add sodium tungstate solution with stannous chloride, reduce remaining ferric iron with titanium trichloride again, to occurring stable blueness, finally use potassium bichromate solution residual titration to colourless, analytic process complex operation, is not suitable for the express-analysis of ore leachate in enormous quantities equally.
The inventive method adopts the oxygenant fast processing ore leachate that a kind of environmental pollution is little, the copper in iodometric determination ore leachate.In the solution of measuring after copper, add suitable reagent, simplify analytic process, then use the iron in iodometric determination ore leachate, thereby realize the Fast Continuous Determination to copper iron in ore leachate.
Summary of the invention
The object of the present invention is to provide that a kind of environmental pollution is little, quick, easy, easy operating and there is good accuracy and the Fast Continuous Determination ore leachate of precision in the method for copper iron.
For achieving the above object, the present invention is by the following technical solutions:
In Fast Continuous Determination ore leachate, a method for copper iron, is characterized in that, comprises the following steps:
A. get 5 ~ 10mL ore leachate to be measured, add low-temperature heat after oxygenant, to volume be 1 ~ 2mL;
B. after being cooled to room temperature, regulate acidity, add screening agent and shelter iron, add afterwards potassium iodide, make indicator with starch, with sodium thiosulfate standard solution titration copper;
C. to adding the demasking agent iron that demasks in the solution of measuring after copper, place;
D. use sodium thiosulfate standard solution titration iron, analyze and do reagent blank simultaneously, the actual iron loss sodium thiosulfate standard solution volume of surveying deducts reagent blank for consuming sodium thiosulfate standard solution volume.
Method as above, preferably, the oxygenant described in step a is hydrogen peroxide, and concentration is 30wt%, and addition is 1.0 ~ 3.0mL.Its objective is the reducing substanceses such as the ferrous iron in oxidized ore leachate.
Method as above, preferably, the temperature of the low-temperature heat described in step a is 60 ~ 100 ℃.Object is to guarantee that hydrogen peroxide by reducing substances oxidations such as the ferrous irons in ore leachate completely.
Method as above, preferably, the adjusting acidity described in step b is to add the acetic acid-ammonium acetate buffer solution of pH ≈ 5 to regulate acidity.
Method as above, preferably, the addition of the acetic acid-ammonium acetate buffer solution of described pH ≈ 5 for adding until solution redness no longer deepen and excessive 2mL.
Method as above, preferably, the screening agent described in step b is ammonium bifluoride saturated solution, shelters completely and excessive 0.5 ~ 1.0mL.
Method as above, preferably, the addition of the potassium iodide described in step b is 1 ~ 2g.
Method as above, preferably, the hydrochloric acid solution that the demasking agent described in step c is aluminium choride, addition is 5.0 ~ 10.0mL.
Method as above, preferably, the compound method of the hydrochloric acid solution of described aluminium choride is: 500gAlCl
36H
2o, adds 150mL HCl, rare to 1000mL, mixes for subsequent use.
Method as above, preferably, be 3 ~ 5min the standing time described in step c.Because the hydrochloric acid solution acidity of aluminium choride is larger, the reaction of demasking is very fast, and in the short time, reaction can be completely.
The invention has the advantages that: by adding a certain amount of hydrogen peroxide to process ore leachate, shortened analysis minute, avoided using strong acid, reduced the pollution to environment.The inventive method environmental pollution is little, quick, operating process is easy to control and easily grasp, and is therefore more applicable for analysis and the mensuration of copper iron in ore leachate in enormous quantities, and acquired results has good accuracy and precision.
Below by embodiment, the invention will be further described, but and do not mean that limiting the scope of the invention.
Specific implementation method
The invention provides the method for copper iron in a kind of Fast Continuous Determination ore leachate, the steps include: to pipette a certain amount of ore leachate in container, add a certain amount of hydrogen peroxide, low-temperature heat ore leachate, to volume be 1 ~ 2mL, be cooled to room temperature, by the acetic acid-ammonium acetate buffer solution adjusting acidity of pH ≈ 5, make the ferric ion in solution generate ferric acetate simultaneously, shelter iron with ammonium bifluoride, add potassium iodide, make indicator with starch, be titrated to blueness with sodium thiosulfate standard solution and disappear, calculate copper ion concentration with this.To adding the aluminium choride iron that demasks in the solution of measuring after copper, place, be titrated to blue disappearance with sodium thiosulfate standard solution, calculate iron concentration with this.
Embodiment 1
Pipette 5.00mL ore leachate in 250mL conical flask, add 2.0mL hydrogen peroxide, low-temperature heat ore leachate, to volume be 1 ~ 2mL, be cooled to room temperature, no longer deepen and excessive 2mL to acetic acid-ammonium acetate buffer solution to the redness that drips pH ≈ 5 in solution, then drip ammonium bifluoride saturated solution and disappear and excessive 0.5mL to red, with a small amount of water washing bottle wall, shake up, in solution, add 1 ~ 2g potassium iodide, shake up.Rapidly by the sodium thiosulfate standard solution (titer of standard solution: fCu=1.5836mg/mL; FFe=1.3917mg/mL) be titrated to faint yellow.Add 1mL5g/L starch solution, continue to be titrated to blue disappearance just, be terminal.Consume sodium thiosulfate standard solution 7.17mL, in solution, copper ion concentration is 2.27g/L.To the hydrochloric acid solution that adds 8.0mL aluminium choride in the solution of measuring after copper along bottle wall, with a small amount of water washing bottle wall, shake up.Being titrated to blue disappearance with sodium thiosulfate standard solution is terminal.Consume sodium thiosulfate standard solution 9.39mL, deduct reagent blank 0.30mL, actual survey iron loss sodium thiosulfate standard solution is 9.09mL, and in solution, iron concentration is 2.53g/L.
Embodiment 2
Pipette 10.00mL ore leachate in 100mL volumetric flask, be diluted to scale, shake up, divide and get 10.00mL solution in 250mL conical flask, add 2.0mL hydrogen peroxide, low-temperature heat ore leachate, to volume be 1 ~ 2mL, be cooled to room temperature, no longer deepen and excessive 2mL to acetic acid-ammonium acetate buffer solution to the redness that drips pH ≈ 5 in solution, then drip ammonium bifluoride saturated solution and disappear and excessive 0.5mL to red, with a small amount of water washing bottle wall, shake up, in solution, add 1 ~ 2g potassium iodide, shake up.Rapidly with sodium thiosulfate standard solution (fCu=1.5836mg/mL; FFe=1.3917mg/mL) be titrated to faint yellow.Add 1mL5g/L starch solution, continue to be titrated to blue disappearance just, be terminal.Consume sodium thiosulfate standard solution 4.09mL, in solution, copper ion concentration is 6.48g/L.To the hydrochloric acid solution that adds 9.0mL aluminium choride in the solution of measuring after copper along bottle wall, with a small amount of water washing bottle wall, shake up.Being titrated to blue disappearance with sodium thiosulfate standard solution is terminal.Consume sodium thiosulfate standard solution 26.15mL, deduct reagent blank 0.30mL, actual survey iron loss sodium thiosulfate standard solution is 25.85mL, and in solution, iron concentration is 35.98g/L.
Embodiment 3
Pipette 10.00mL ore leachate in 100mL volumetric flask, be diluted to scale, shake up, divide and get 10.00mL solution in 250mL conical flask, add 2.0mL hydrogen peroxide, low-temperature heat ore leachate, to volume be 1 ~ 2mL, be cooled to room temperature, no longer deepen and excessive 2mL to acetic acid-ammonium acetate buffer solution to the redness that drips pH ≈ 5 in solution, then drip ammonium bifluoride saturated solution and disappear and excessive 0.5mL to red, with a small amount of water washing bottle wall, shake up, in solution, add 1 ~ 2g potassium iodide, shake up.Rapidly with sodium thiosulfate standard solution (fCu=1.5836mg/mL; FFe=1.3917mg/mL) be titrated to faint yellow.Add 1mL5g/L starch solution, continue to be titrated to blue disappearance just, be terminal.Consume sodium thiosulfate standard solution 11.95mL, in solution, copper ion concentration is 18.92g/L.To the hydrochloric acid solution that adds 10.0mL aluminium choride in the solution of measuring after copper along bottle wall, with a small amount of water washing bottle wall, shake up.Being titrated to blue disappearance with sodium thiosulfate standard solution is terminal.Consume sodium thiosulfate standard solution 2.30mL, deduct reagent blank 0.30mL, actual survey iron loss sodium thiosulfate standard solution is 2.00mL, and in solution, iron concentration is 2.78g/L.
Standard method
Iodimetric titration is surveyed copper in ore leachate: pipette 5.00mL ore leachate in 250mL conical flask, add 5mL nitric acid and 3mL sulfuric acid, on electric furnace, heating evaporation to the white cigarette of sulfuric anhydride emits to the greatest extent, be cooled to room temperature, with 20mL water washing bottle wall, be placed on electric hot plate and boil, salt is dissolved completely, take off, be cooled to room temperature, no longer deepen and excessive 2mL to acetic acid-ammonium acetate buffer solution to the redness that drips pH ≈ 5 in solution, then dripping ammonium bifluoride saturated solution disappears and excessive 1.0mL to red, with a small amount of water washing bottle wall, shake up, in solution, add 2 ~ 3g potassium iodide, shake up.Rapidly with sodium thiosulfate standard solution (fCu=1.5836mg/mL; FFe=1.3917mg/mL) be titrated to faint yellow.Add 1mL5g/L starch solution, continue to be titrated to blue disappearance just, be terminal.Consume sodium thiosulfate standard solution 7.23mL, in solution, copper ion concentration is 2.29g/L.
Dichromate method is surveyed iron in ore leachate: pipette 5.00mL ore leachate in 250mL conical flask, a small amount of water washing bottle wall, be heated to closely boil, drip while hot stannous chloride solution and (take 5g stannous chloride, add 10mL1+1 hydrochloric acid (hydrochloric acid that refers to 36-38wt% adds isopyknic water dilution), heating for dissolving, is diluted to 100mL.Used time now joins), and fully shake, be light yellow to solution, be cooled to room temperature with flowing water immediately.Add 1mL250g/L sodium tungstate solution, shake limit, limit drips 20+80 titanium trichloride solution (refer to that the titanium trichloride solution of 15wt% adds the water dilution of 4 times of volumes, the used time now joins) to the yellow of solution and takes off, and occurs stable blueness, a small amount of water washing bottle wall.With extremely colourless (not remembering reading) of 0.5g/L potassium bichromate solution readjustment solution.Add immediately 20mL sulfuric acid, phosphoric acid mixed solution (under constantly stirring, slowly adding 150mL sulfuric acid and 150mL phosphoric acid in 700mL water) and 2 5g/L diphenylamine sulfonic acid sodium solutions, with potassium dichromate standard solution (fFe
2+=2.0000mg/mL) volumetric soiutions is to stablize purple be terminal.Consume potassium dichromate standard solution 6.32mL, in solution, iron concentration is 2.53g/L.
Veracity and precision experiment
Method described in employing embodiment 1 and standard method are analyzed and are measured the veracity and precision of making a concrete analysis of the inventive method copper iron concentration in ore leachate 1 ~ 5# respectively.The inventive method is to copper iron concentration replicate determination 6 times (n=6) in ore leachate, the data that record are done to mathematics statistical treatment, in ore leachate, copper ion concentration relative standard deviation is in 0.26 ~ 0.65% scope, in ore leachate, iron concentration relative standard deviation is in 0.23 ~ 1.61% scope, and experimental result refers to table 1 ~ 2.From result, utilize the inventive method to analyze to measure to copper iron concentration in ore leachate and there is good accuracy and precision.
Copper ion concentration veracity and precision experiment in table 1 ore leachate
Iron concentration veracity and precision experiment in table 2 ore leachate
Claims (10)
1. a method for copper iron in Fast Continuous Determination ore leachate, is characterized in that, comprises the following steps:
A. get 5 ~ 10mL ore leachate to be measured, add low-temperature heat after oxygenant, to volume be 1 ~ 2mL;
B. after being cooled to room temperature, regulate acidity, add screening agent and shelter iron, add afterwards potassium iodide, make indicator with starch, with sodium thiosulfate standard solution titration copper;
C. to adding the demasking agent iron that demasks in the solution of measuring after copper, place;
D. use sodium thiosulfate standard solution titration iron, analyze and do reagent blank simultaneously, the actual iron loss sodium thiosulfate standard solution volume of surveying deducts reagent blank for consuming sodium thiosulfate standard solution volume.
2. the method for claim 1, is characterized in that, the oxygenant described in step a is hydrogen peroxide, and concentration is 30wt%, and addition is 1.0 ~ 3.0mL.
3. the method for claim 1, is characterized in that, the temperature of the low-temperature heat described in step a is 60 ~ 100 ℃.
4. the method for claim 1, is characterized in that, the adjusting acidity described in step b is to add the acetic acid-ammonium acetate buffer solution of pH ≈ 5 to regulate acidity.
5. method as claimed in claim 4, is characterized in that, the addition of the acetic acid-ammonium acetate buffer solution of described pH ≈ 5 for adding until solution redness no longer deepen and excessive 2mL.
6. the method for claim 1, is characterized in that, the screening agent described in step b is ammonium bifluoride saturated solution, shelters completely and excessive 0.5 ~ 1.0mL.
7. the method for claim 1, is characterized in that, the addition of the potassium iodide described in step b is 1 ~ 2g.
8. the method for claim 1, is characterized in that, the hydrochloric acid solution that the demasking agent described in step c is aluminium choride, and addition is 5.0 ~ 10.0mL.
9. method as claimed in claim 6, is characterized in that, the compound method of the hydrochloric acid solution of described aluminium choride is: 500g AlCl
36H
2o, adds 150mL HCl, rare to 1000mL, mixes for subsequent use.
10. the method for claim 1, is characterized in that, be 3 ~ 5min the standing time described in step c.
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Cited By (8)
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| CN104792931A (en) * | 2015-05-05 | 2015-07-22 | 梧州市产品质量检验所 | Method of detecting copper content in metallic ores |
| CN104792930A (en) * | 2015-05-05 | 2015-07-22 | 梧州市产品质量检验所 | Detection method for copper content of crude copper alloy |
| CN105467068A (en) * | 2015-12-24 | 2016-04-06 | 阳谷祥光铜业有限公司 | Method for detecting copper, iron and calcium in flash converting furnace slag |
| CN106404991A (en) * | 2016-08-23 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Method for determination of iron in copper alloy |
| CN112504909A (en) * | 2020-11-07 | 2021-03-16 | 韶关凯鸿纳米材料有限公司 | Method for measuring ammonium bicarbonate content and zinc oxide production process for controlling ammonium bicarbonate dosage |
| CN113049736A (en) * | 2021-03-11 | 2021-06-29 | 青海西钢特殊钢科技开发有限公司 | Method for determining nickel in nickel-chromium pig iron smelted in blast furnace |
| CN113049738A (en) * | 2021-03-23 | 2021-06-29 | 湖北三鑫金铜股份有限公司 | Method for rapidly determining iron content in copper ore |
| CN114544860A (en) * | 2022-03-14 | 2022-05-27 | 昆明理工大学 | Method for measuring contents of elemental copper, copper ions, ferrous ions and ferric ions in copper slag |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792931A (en) * | 2015-05-05 | 2015-07-22 | 梧州市产品质量检验所 | Method of detecting copper content in metallic ores |
| CN104792930A (en) * | 2015-05-05 | 2015-07-22 | 梧州市产品质量检验所 | Detection method for copper content of crude copper alloy |
| CN105467068A (en) * | 2015-12-24 | 2016-04-06 | 阳谷祥光铜业有限公司 | Method for detecting copper, iron and calcium in flash converting furnace slag |
| CN106404991A (en) * | 2016-08-23 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Method for determination of iron in copper alloy |
| CN112504909A (en) * | 2020-11-07 | 2021-03-16 | 韶关凯鸿纳米材料有限公司 | Method for measuring ammonium bicarbonate content and zinc oxide production process for controlling ammonium bicarbonate dosage |
| CN113049736A (en) * | 2021-03-11 | 2021-06-29 | 青海西钢特殊钢科技开发有限公司 | Method for determining nickel in nickel-chromium pig iron smelted in blast furnace |
| CN113049738A (en) * | 2021-03-23 | 2021-06-29 | 湖北三鑫金铜股份有限公司 | Method for rapidly determining iron content in copper ore |
| CN114544860A (en) * | 2022-03-14 | 2022-05-27 | 昆明理工大学 | Method for measuring contents of elemental copper, copper ions, ferrous ions and ferric ions in copper slag |
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Application publication date: 20140702 |